EP0061411B1 - Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall - Google Patents

Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall Download PDF

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Publication number
EP0061411B1
EP0061411B1 EP82420037A EP82420037A EP0061411B1 EP 0061411 B1 EP0061411 B1 EP 0061411B1 EP 82420037 A EP82420037 A EP 82420037A EP 82420037 A EP82420037 A EP 82420037A EP 0061411 B1 EP0061411 B1 EP 0061411B1
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EP
European Patent Office
Prior art keywords
injection
ccl
process according
halogenated
substance
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82420037A
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English (en)
French (fr)
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EP0061411A1 (de
Inventor
Gilbert Pollet
Pierre Du Manoir
Pierre Guerit
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Servimetal SA
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Servimetal SA
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Application filed by Servimetal SA filed Critical Servimetal SA
Priority to AT82420037T priority Critical patent/ATE20541T1/de
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • C22B21/064—Obtaining aluminium refining using inert or reactive gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ

Definitions

  • the present invention relates to a process for the precise injection, into a liquid metal, of halogenated derivatives, liquid or in solution.
  • the present invention belongs to this second category. Indeed, the handling and use of chlorine in foundry workshops poses safety, hygiene, pollution and corrosion problems which encourage us to seek other solutions.
  • anhydrous metal chlorides such as TiCl 4 , AICI 3 , MnCl 2 , and organic derivatives such as CCL 4 (carbon tetrachloride), C Z CI 4 (perchlorethylene) or C 2 CI 6 have been used. (hexachlorethane).
  • This product which is solid at room temperature, sublimes around 187 ° C. For this reason, it is usually introduced into aluminum in the form of pellets placed in a chamber through which the liquid metal passes, or, by means of a perforated bell, made of graphite, which is lowered, into the metal. liquid.
  • a perforated bell, made of graphite which is lowered, into the metal. liquid.
  • its volatilization and thermal cracking are extremely rapid and require little more than 2 to 3 minutes. But this speed excludes any possibility of precise dosing and, above all, of continuous action on a stream of liquid aluminum.
  • the doses used are much greater than the quantity actually necessary, the excess requires effective capture.
  • the object of the present invention is a precise and continuous injection process into a liquid metal of a halogenated substance, liquid at room temperature formed by at least one defined chemical compound, consists of carbon and at least one halogen. chosen from chlorine and fluorine, and having a halogen / carbon ratio at least equal to 2 and preferably between 2 and 4, such as perchlorethylene, hexachloretane, carbon tetrachloride and chlorofluorinated derivatives: CCl 3 F , CCI3 CF3, CCl 3 CClF 2 , CCI Z F-CCIF 2 , CCl 2 F-CCl 2 F, CCl 3 - CClF 2 , CCl 3 -CCl 2 F, and optionally with an anhydrous metal halide such as TiCI 4 or BCl 3 .
  • an anhydrous metal halide such as TiCI 4 or BCl 3 .
  • said halogenated substance is removed from a tank, it is introduced by means of a metering pump, into a vaporizer brought to a temperature at least equal to the vaporization temperature of said substance under the injection pressure, and it is entrained, in the vapor state, by a current of inert gas, towards an injection means opening into the liquid metal.
  • halogenated substance at least one defined chemical compound, composed of carbon and at least one halogen chosen from chlorine and fluorine.
  • the single figure shows a device for putting the process into service. It consists of: a tank (1) fitted with a tight cover (2), a closable adjustment (3) for filling, a level gauge (4); a sampling tube (5), fitted with a shut-off valve (6), is connected to a piston metering micropump (7) which can collect and precisely inject the halogenated substance (8), to a rate which can be, for example, between 0.1 and 10 milliliters per minute, without these values constituting a limitation of the invention.
  • the liquid halogenated substance (8) passes through a non-return valve (9) and enters the vaporizer (10) provided with a regulated and thermostatically controlled heating means (11), of any known type, for example with electrical resistance.
  • An inert gas such as nitrogen, argon or helium, taken from the pressurized storage means (12) using a pressure reducer (13) and a flow meter (14), also enters the vaporizer where it mixes to the vapors of the halogenated substance and carries them through the injection pipe (15) to the injection means (16) which can be, for example, a graphite rod, immersed in the liquid metal (17) passing through the processing pocket (18).
  • nitrogen, argon or helium taken from the pressurized storage means (12) using a pressure reducer (13) and a flow meter (14), also enters the vaporizer where it mixes to the vapors of the halogenated substance and carries them through the injection pipe (15) to the injection means (16) which can be, for example, a graphite rod, immersed in the liquid metal (17) passing through the processing pocket (18).
  • a variant of the apparatus for higher flow rates of treatment gas, consists in adding to the system described above, an additional flow rate of gas: nitrogen, argon or helium, introduced downstream of the vaporizer (10) by a nozzle (24) on the pipe (15); this allows, in the operating range of the micro-pump, to ensure the desired amount of halogen with a predetermined dilution level without passing the entire gas flow through the vaporizer.
  • This solution has the advantage of a higher chlorine content by weight than that of pure C Z CI 4 , while retaining the advantage of the liquid state, which allows its precise injection by a metering pump. If you want to keep the mixture in its liquid state at temperatures close to ambient, you can introduce up to about 500 grams / liter of C 2 Cl 6 .
  • a solution was chosen containing from 0.1 to 30% and, preferably, from 15 to 20 % by weight of C 2 Cl 6 .
  • the halogenated substance can also consist, partially or wholly, of chlorofluorinated derivatives, and in particular CCl 3 F, CCl 3 - CF 3 , CCl 2 F-CClF 2 , CCl 3 CCIFZ, CCLF-CCI, F, CCl 3 CCl 2 F, the boiling points of which range between 24 and 138 ° C.
  • TiCl 4 titanium tetrachloride
  • BCI 3 boron trichloride
  • the injection pump is a positive displacement piston pump designed to precisely deliver small volumes of predetermined liquid and with a reliability of + 1% by volume.
  • a diaphragm pump could also be used.
  • the vaporizer preferably comprises a spiral tube or a bundle of parallel tubes, so that the halogenated substance and the carrier gas can exit therefrom at a temperature which can reach 200 ° C. and even beyond, if it is necessary, but sufficient to avoid any condensation and which must be adapted to the halogenated derivative chosen and to the pressure under which the injection is carried out.
  • Heating is provided by an electric resistance regulated from a temperature sensor arranged on the path of the gases leaving the vaporizer.
  • the injection into the liquid metal can be carried out by various known means, for example, by a graphite rod (16) disposed in the upstream compartment (19) of the treatment bag (18) into which the metal to be purified arrives or by a porous plug (20) placed at the bottom of the pocket according to a well-known technique (French patent FR No. 1,031,504).
  • the downstream compartment (21) is separated from the upstream compartment by a partition (22) and it may include any known filtration means such as alumina beads or granules (23).
  • the injection can also be carried out in rotary devices such as the “Spinning Nozzle Inert flotation System” (SNIF) of Union CARBIDE (US patent 3,870,511) as a replacement for the injection of chlorine, or in devices similar to propeller or turbine, in which the arrival of the halogenated vapors and the carrier gas is done by the axis.
  • rotary devices such as the “Spinning Nozzle Inert flotation System” (SNIF) of Union CARBIDE (US patent 3,870,511) as a replacement for the injection of chlorine, or in devices similar to propeller or turbine, in which the arrival of the halogenated vapors and the carrier gas is done by the axis.
  • the metal is continuously treated in passing, by injection of the halogenated substance.
  • An injection device was constructed, according to the diagram in the figure, comprising a 10-liter reservoir, of a mixture at 80% by weight of perchlorethylene and 20% by weight of exaclorethane.
  • the dosing micropump has an adjustable flow rate between 1 and 10 milliliters / minute.
  • the vaporizer is preheated to (280 ⁇ 5 ° C).
  • the carrier gas is nitrogen, injected under a pressure of 2.5 bars and a flow rate of 2 m3 / hour.
  • the amount of perchlorethylene-hexachlorethane mixture was adjusted to 250 milliliters / hour corresponding to 100 grams of chlorine for a flow rate of aluminum, in the treatment bag, of 2 tonnes / hour.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Lubricants (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Catching Or Destruction (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Seal Device For Vehicle (AREA)

Claims (6)

1. Verfahren zum genauen und kontinuierlichen Einblasen einer bei Raumtemperatur flüssigen Halogenverbindung, die aus wenigstens einer definierten chemischen Verbindung gebildet ist, die aus Kohlenstoff und wenigstens einem unter Chlor und Fluor gewählten Halogen mit einem Halogen/ Kohlenstoff-Verhältnis von mindestens 2 und vorzugsweise im Bereich von 2 bis 4, wie Perchlorethylen, Hexachlorethan, Tetrachlorkohlenstoff und den Chlor-Fluor-Abkömmlingen: CCIaF, CCla-CF2, CCl3 CClF2, CCl2 CClF2, CCL2F-CCI2F, CCl3 CClF2, CCl3 CCl2F, zusammengesetzt ist und ggf. einen Zusatz eines wasserfreien Metallhalogenids, wie z.B. TiCl4, aufweist, in eine Metallschmelze, dadurch gekennzeichnet, dass man die Halogenverbindung einem Behälter entnimmt, dass man sie mittels einer Dosierpumpe in einen Verdampfer einführt, der auf eine der Verdampfungstemperatur dieser Verbindung beim Einblasdruck wenigstens gleiche Temperatur gebracht ist, und dass man sie im Dampfzustand durch einen Inertgasstrom zu einem in der Metallschmelze mündenden Einblasmittel fördert.
2. Einblasverfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Intergas stromauf des Verdampfers eingeführt wird.
3. Einblasverfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Inertgas teilweise stromauf und teilweise stromab des Verdampfers eingeführt wird.
4. Einblasverfahren nach irgendeinem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Einblasmittel in einer vom Metallschmelzenstrom durchströmten Pfanne angeordnet ist.
5. Einblasverfahren nach irgendeinem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass das Einblasmittel in einem Tiegel oder in einem Beckenofen angeordnet ist.
6. Einblasverfahren nach irgendeinem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Halogenverbindung aus einer Lösung von Hexachlorethan in Perchlorethylen mit einer Konzentration im Bereich von 0,1 bis 30 Gew.-% Hexachlorethan und vorzugsweise im Bereich von 15 bis 20% besteht.
EP82420037A 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall Expired EP0061411B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82420037T ATE20541T1 (de) 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen einblasen einer gasfoermigen halogenverbindung in fluessiges metall.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8106134 1981-03-23
FR8106134A FR2502181B1 (fr) 1981-03-23 1981-03-23 Procede et appareillage pour l'injection precise et continue d'un derive halogene a l'etat gazeux dans un metal liquide

Publications (2)

Publication Number Publication Date
EP0061411A1 EP0061411A1 (de) 1982-09-29
EP0061411B1 true EP0061411B1 (de) 1986-06-25

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ID=9256686

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EP82420037A Expired EP0061411B1 (de) 1981-03-23 1982-03-19 Verfahren zum genauen und kontinuierlichen Einblasen einer gasförmigen Halogenverbindung in flüssiges Metall

Country Status (16)

Country Link
US (1) US4402741A (de)
EP (1) EP0061411B1 (de)
JP (1) JPS57164945A (de)
KR (1) KR830008767A (de)
AT (1) ATE20541T1 (de)
AU (1) AU541804B2 (de)
BR (1) BR8201584A (de)
CA (1) CA1180164A (de)
DE (1) DE3271823D1 (de)
DK (1) DK127382A (de)
ES (1) ES8306803A1 (de)
FR (1) FR2502181B1 (de)
GR (1) GR76038B (de)
HU (1) HU186486B (de)
NO (1) NO820940L (de)
YU (1) YU59782A (de)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4552667A (en) * 1984-06-25 1985-11-12 Shultz Clifford G Destruction of organic hazardous wastes
US4666696A (en) * 1985-03-29 1987-05-19 Detox International Corporation Destruction of nerve gases and other cholinesterase inhibitors by molten metal reduction
JPS6274030A (ja) * 1985-09-27 1987-04-04 Showa Alum Corp アルミニウム溶湯の処理方法
US4770697A (en) * 1986-10-30 1988-09-13 Air Products And Chemicals, Inc. Blanketing atmosphere for molten aluminum-lithium alloys or pure lithium
US4959101A (en) * 1987-06-29 1990-09-25 Aga Ab Process for degassing aluminum melts with sulfur hexafluoride
US5090998A (en) * 1989-12-20 1992-02-25 Alusuisse-Lonza Services Ltd. Purification of metal melts with halogen gas generated in an electrolysis cell
FR2669041B1 (fr) * 1990-11-09 1994-02-04 Sfrm Procede pour le traitement d'un metal en fusion et son transfert dans un espace recepteur et systeme pour la mise en óoeuvre de ce procede.
US5935295A (en) * 1997-10-16 1999-08-10 Megy; Joseph A. Molten aluminum treatment
AU2003278765A1 (en) * 2002-09-07 2004-04-08 International Titanium Powder, Llc. Method and apparatus for controlling the size of powder produced by the armstrong process
WO2004022800A1 (en) 2002-09-07 2004-03-18 International Titanium Powder, Llc. Process for separating ti from a ti slurry
AU2003263082A1 (en) 2002-10-07 2004-05-04 International Titanium Powder, Llc. System and method of producing metals and alloys
US20070017319A1 (en) 2005-07-21 2007-01-25 International Titanium Powder, Llc. Titanium alloy
WO2007044635A2 (en) 2005-10-06 2007-04-19 International Titanium Powder, Llc Titanium or titanium alloy with titanium boride dispersion
US7753989B2 (en) 2006-12-22 2010-07-13 Cristal Us, Inc. Direct passivation of metal powder
US9127333B2 (en) 2007-04-25 2015-09-08 Lance Jacobsen Liquid injection of VCL4 into superheated TiCL4 for the production of Ti-V alloy powder

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2085697A (en) * 1933-08-05 1937-06-29 Nat Smelting Co Method for treating aluminum and aluminum alloys
US1998467A (en) * 1934-06-30 1935-04-23 Aluminum Co Of America Method of treating aluminum-base alloys
US2447672A (en) * 1944-11-20 1948-08-24 American Smelting Refining Apparatus for chloridizing aluminum-base alloys
FR1463079A (fr) * 1965-10-21 1966-06-03 Air Liquide Procédé de traitement des métaux liquides, applicable notamment à l'élaboration de fonte nodulaire
CH494282A (de) * 1968-02-23 1970-07-31 Alusuisse Verfahren zum Behandeln von Metallschmelzen mit gasförmigen Stoffen
US3972709A (en) * 1973-06-04 1976-08-03 Southwire Company Method for dispersing gas into a molten metal
US3854934A (en) * 1973-06-18 1974-12-17 Alusuisse Purification of molten aluminum and alloys
US3958980A (en) * 1974-11-08 1976-05-25 Union Carbide Corporation Process for removing alkali-metal impurities from molten aluminum
JPS5223514A (en) * 1975-08-19 1977-02-22 Showa Denko Kk Treatment method for metal melt
JPS5819589B2 (ja) * 1976-03-29 1983-04-19 三菱電機株式会社 エレベ−タのドアレ−ル
JPS5652457Y2 (de) * 1977-08-27 1981-12-07
US4149615A (en) * 1977-09-15 1979-04-17 Westinghouse Electric Corp. Apparatus for mounting an elevator door operator
JPS5917719B2 (ja) * 1978-02-02 1984-04-23 三菱電機株式会社 自動ドア−の安全装置

Also Published As

Publication number Publication date
ES510623A0 (es) 1983-06-01
CA1180164A (fr) 1985-01-02
NO820940L (no) 1982-09-24
US4402741A (en) 1983-09-06
FR2502181B1 (fr) 1985-09-27
ES8306803A1 (es) 1983-06-01
FR2502181A1 (fr) 1982-09-24
KR830008767A (ko) 1983-12-14
DK127382A (da) 1982-09-24
EP0061411A1 (de) 1982-09-29
YU59782A (en) 1985-03-20
HU186486B (en) 1985-08-28
AU541804B2 (en) 1985-01-17
GR76038B (de) 1984-08-03
BR8201584A (pt) 1983-02-08
DE3271823D1 (en) 1986-07-31
JPS57164945A (en) 1982-10-09
ATE20541T1 (de) 1986-07-15
AU8176882A (en) 1982-09-30

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